Process of making asphalt



Patented June-21, 1938 UNITED STATES PATENT OFFICE 2.121.431 rnocrss orMAKING ASPHALT No Drawing. Application February 12, 1937, Serial No.125,428

9 Claims. (Cl. iec -w This invention relates to the manufacture ofasphalt; and it is among the objects of the invention to provide aprocess making possible faster operation than that customary inasphaltmaking, and capable of giving superior products. Other objectsand advantages will appear as the description proceeds.

To the accomplishment of the foregoing and related ends, the invention,then, comprises the m, features hereinafter fully described, andparticularly pointed out in the claims, the following descriptionsetting forth in detail certain illustrative embodiments of theinvention, these being indicative however, of but a few of the various15 ways in which the principle of the invention may be employed.

The raw material may be the stocks customary, in general a petroleumresiduum or the residue left after the vaporizable hydrocarbons through20 the range of lubricating fractions have been taken oil. The rawmaterial, in accordance with the invention, is subjected to the actionof heat and oxidizing conditions, and while oxygen gas may be used. inpractice air is generally more 5 desirable, and such gaseous agent maybe introduced into the residuum to accomplish both the oxidation andagitation, as by air-blowing, while at the same time carrying aparticular catalyst.

In accordance with the invention, the latter is at! an inorganicgasiform agent, or at least'capable of being carried along by an airstream, and containing an acid-forming element such as sulphur orahalogen, and selected from the group consisting of Selene-sulphide, SeS,thlonyl perchloride, SOClz, sulphuric oxyfluoride, $021 2,

ghosphorus oxychloride, POCla, phosphorus oxyuoride, POFa, phosphorusthiofluoride, PSFz, and sillco-fluoroform, SiHFa. Particularly desirableare the halogen-containing compounds, 40 and especially thephosphorus-halogen compounds.

These catalysts are notably effective, and are employed in small amount,as for instance .0001-1 per cent, and where an air stream is employed 45as the primary reagent, the catalyst may be proportionally fed alongtherewith. The temperature of treatment is in general 400 to 550 B.

As a further refinement, particularly advantageous in some instances,the residuum may be 50 air-blown or oxidized by heating at 400-550" F.

with oxygen or air alone without the catalyst to partial conversion todesired specifications, and

then the catalyst is fed in with the air and the reaction is completedto the final desired specifications of melting point, pepetration, etc.

As an example: 1000 barrels of petroleum residuum, obtained by vacuumreduction of Mid-Continent crude, and having a penetration of 200 at 77F., is charged into a tank-which may be suitably equipped with an airspray in the bottom. Air is blown in at the rate of about 50,000 cubicfeet per hour. The temperature of the material rises during theoxidation to about 500 and the treatment is carried on until thepenetration of the material is about 100 at 77 F. 10 At this point,phosphorus oxychloride is admitted along with the air in amount of 0.5per cent by volume, until the material reaches a penetration of about 50at 77 F. The air and catalyst is then stopped, and the material ispumped to storage or shipping containers.

As another example: Petroleum residuum similarly is agitated and blownwith air containing about 0.5 per cent by volume of phosphorusoxychloride, the temperature being maintained at around 500 F., and thetreatment continued until-the material reaches a penetration of about 50at 77 F. The time of treatment may be around eight hours.

As another example: Petroleum residuum is similarly agitated and blownwith air carrying phosphorus oxyflouride as catalyst,- until the productsamples to the desired penetration.

As another example: Residuum similarly is agitated and air blown, withsupply oi sulphur oxyfiuoride as catalyst.

As another example: Residuum similarly is agitated and blown with aircarrying phosphorus thiofluoride as catalyst.

As another example: Residuum similarly is agitated and blown with aircarrying selenosulphide as catalyst.

As another example: Instead of starting with the catalyst .as in theimmediately preceding examples, the residuum is first air blown withouta catalyst, until the penetration is about 100 at 77 F. Then either ofthe catalysts noted is introduced with the air, and the treatmentcontinued until the product shows a penetration of about at 77 F. 5

As another example: Residuum is oxidized with air blowing, until thematerial shows a penetration of at 77 F., then the gaseous catalyst,carried by air, is mixed with the asphalt for a period of about half anhour, the temperature 50 being maintained at around 500 F.

Other types of blowing equipment, aside from the tank mentioned. may beemployed, those such 7 as in my Patents Nos. 1,982,920, 1,950,900 and2,002,670 being especially advantageous. 5a

Other modes of applying the principle of the invention may be employed,change being made as regards the details described, provided thefeatures stated in any of the following claims, or the equivalent orsuch, be employed.

1 therefore particularly point out and distinctly claim as myinventlon:-

1. A process oi. making asphalt, which comprises heating and agitatingpetroleum residuum, at a temperature of 400-550 F.. in exposure to agaseous medium providing oxygen, while transmitting with said gaseousmedium into contact with the petroleum residuum a small amount or acatalyst containing an acid-forming element selected from the groupconsisting 'of selenosulphide, thionyl perchloride, sulphuricoxyfluoride, phosphorus oxychloride, phosphorus oxyiluoride, phosphorusthiotluoride, and silico-fluoroiorm.

2. A process of making asphalt, which comprises heating and agitatingpetroleum residuum, at a temperature of Mil-550 F., in exposure to agaseous medium providing oxygen, until the penetration-test oi thematerial is about 100 at 77 F., then supplying to the residuum a gaseousvmedium providing oxygen and carrying a gasitorm catalyst containing anacid-forming element selected from the group consisting ofselenosulphide, thionyl perchloride, sulphuric oxyfluoride, phosphorusoxychloride, phosphorus 01wfluorlde, phosphorus thiofluoride, andsilico-fluoroform.

3. A process of making asphalt, which comprises heating and agitatingpetroleum residuum, at a temperature of 400-550" R, in exposure to agaseous medium providing oxygen, until the material is partly convertedto desired specification, and then completing the treatment by turtherblowing with a gaseous medium providing oxygen and carrying a smallamount of a catalyst containing an acid-forming element selected fromthe group consisting of seleno-sulphide, thionyl perchloride, sulphuricoxyfluoride, phosphorus oxychloride, phosphorus oxyfluoride, phosphorusthioiluoride, and silico-fluoroiorm.

1 dQ Aprocess of making asphalt, which comat an oxidizing temperature inexposure to a gaseous medium providing oxygen, while transmitting withsaid gaseous medium in contact with the petroleum a catalytic amount ofphosphorus oxychlorlde.

5. A process of making asphalt, which comprises heating and agitatingpetroleum residuum, at an oxidizing temperature in exposure to a gaseousmedium providing oxygen, while transmitting with said gaseous medium incontact with the petroleum a catalytic amount of phosphorusthioiiuoride. I

6. A process of making asphalt, which comprises heating and agitatingpetroleum residuum, at an oxidizing temperature in exposure to a gaseousmedium providing oxygen, while transmitting with said gaseous medium incontact with the petroleum a catalytic amount of seleno-sulphide.

7. A process of making asphalt, which comprises heating and agitatingpetroleum residuum, at an oxidizing temperature in exposure to a gaseousmedium providing oxygen, until the material is partly converted todesired specification, and then completing the treatment by furtherblowing with a gaseous medium providing oxygen and carrying a catalyticamount of phosphorus oxychloride.

8. A process or making asphalt, which comprises heating and agitatingpetroleum residuum, at an oxidizing temperature in exposure to a gaseousmedium providing oxygen, until the material is partly converted todesired specification, and then completing the treatment by Iurtherblowing with a gaseous medium providing oxygen and carrying a catalyticamount of phosphorus thiofluoride.

9. A process of making asphalt, which comprises heating and agitatingpetroleum residuum, at an oxidizing temperature in exposure to a gaseousmedium providing oxygen, until the material is partly converted todesired specification, and then completing the treatment by furtherblowing with a gaseous medium providing oxygen and carrying a catalyticamount of seleno-sulphide.

ELLIOT! B. McCONNEIL.

